#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/22/2202259.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202259 loop_ _publ_author_name 'Jian-Feng Shi' 'Yan-Guang Wang' _publ_section_title (5aR,8aR,9R)-9-(3,4,5-Trimethoxyphenyl)-5a,6,8a,9-tetrahydrofuro[3',4':6,7]naphtho[2,3-d][1,3]dioxole-5,8-dione _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o756 _journal_page_last o758 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'C22 H20 O8' _chemical_formula_moiety 'C22 H20 O8' _chemical_formula_sum 'C22 H20 O8' _chemical_formula_weight 412.38 _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.4927(9) _cell_length_b 12.1940(11) _cell_length_c 24.9681(18) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.5 _cell_measurement_theta_min 3.0 _cell_volume 1976.8(4) _computing_cell_refinement ; MSC/AFC Diffractometer Control Software ; _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure corporation, 1992) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1993)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997) and CAMERON (Watkin, 1993)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 4509 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 1.6 _diffrn_standards_decay_% 0.2 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.11 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_correction_T_min 0.963 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_meas 1.379 _exptl_crystal_density_method 'flotation in a mixture of hexane and carbontetrachloride' _exptl_crystal_description prism _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.23 _refine_diff_density_min -0.25 _refine_ls_extinction_coef 0.0133(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 0.98 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 272 _refine_ls_number_reflns 2610 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.98 _refine_ls_R_factor_gt 0.033 _refine_ls_shift/su_max <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0667P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.112 _reflns_number_gt 1817 _reflns_number_total 2610 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya6159.cif _[local]_cod_data_source_block I _cod_database_code 2202259 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C2 0.3339(7) -0.2267(3) 0.06118(18) 0.0853(12) Uani d . 1 . . C H2A 0.2786 -0.276 0.0343 0.102 Uiso calc R 1 . . H H2B 0.3792 -0.2699 0.0916 0.102 Uiso calc R 1 . . H C3A 0.4716(6) -0.0592(2) 0.05652(11) 0.0527(8) Uani d . 1 . . C C4 0.5954(5) 0.0284(2) 0.05157(11) 0.0506(7) Uani d . 1 . . C H4 0.7248 0.0222 0.0359 0.061 Uiso calc R 1 . . H C4A 0.5225(5) 0.1307(2) 0.07098(10) 0.0426(6) Uani d . 1 . . C C5 0.6568(5) 0.2269(2) 0.06469(10) 0.0451(6) Uani d . 1 . . C C5A 0.5788(4) 0.3315(2) 0.08826(11) 0.0458(7) Uani d . 1 . . C H5A 0.6144 0.3326 0.1264 0.055 Uiso calc R 1 . . H C6 0.6426(6) 0.4404(3) 0.06363(14) 0.0668(9) Uani d . 1 . . C H6A 0.7728 0.4653 0.0783 0.08 Uiso calc R 1 . . H H6B 0.6551 0.4344 0.025 0.08 Uiso calc R 1 . . H C8 0.3044(6) 0.4577(3) 0.09154(12) 0.0552(8) Uani d . 1 . . C C8A 0.3467(5) 0.3369(2) 0.08316(10) 0.0447(7) Uani d . 1 . . C H8A 0.3161 0.3221 0.0454 0.054 Uiso calc R 1 . . H C9 0.2392(4) 0.2475(2) 0.11477(10) 0.0419(6) Uani d . 1 . . C H9 0.0927 0.25 0.1054 0.05 Uiso calc R 1 . . H C9A 0.3252(5) 0.1386(2) 0.09408(10) 0.0422(6) Uani d . 1 . . C C10 0.2017(5) 0.0453(3) 0.09833(11) 0.0518(7) Uani d . 1 . . C H10 0.0713 0.0489 0.1136 0.062 Uiso calc R 1 . . H C10A 0.2784(5) -0.0513(3) 0.07935(12) 0.0548(8) Uani d . 1 . . C C11 0.2552(4) 0.2596(2) 0.17518(10) 0.0398(6) Uani d . 1 . . C C12 0.1103(4) 0.3232(2) 0.20177(10) 0.0435(6) Uani d . 1 . . C H12 0.0054 0.3569 0.1825 0.052 Uiso calc R 1 . . H C13 0.1204(5) 0.3368(2) 0.25649(11) 0.0470(7) Uani d . 1 . . C C13A -0.1912(6) 0.4404(3) 0.25986(15) 0.0718(10) Uani d . 1 . . C H13A -0.2721 0.4813 0.2851 0.108 Uiso calc R 1 . . H H13B -0.2719 0.381 0.2458 0.108 Uiso calc R 1 . . H H13C -0.1493 0.4876 0.2311 0.108 Uiso calc R 1 . . H C14 0.2758(4) 0.2861(2) 0.28575(10) 0.0463(7) Uani d . 1 . . C C14A 0.1794(6) 0.2143(3) 0.36825(13) 0.0753(10) Uani d . 1 . . C H14A 0.1906 0.2261 0.4062 0.113 Uiso calc R 1 . . H H14B 0.2388 0.1447 0.3592 0.113 Uiso calc R 1 . . H H14C 0.0368 0.215 0.358 0.113 Uiso calc R 1 . . H C15 0.4209(4) 0.2224(2) 0.25943(10) 0.0453(7) Uani d . 1 . . C C15A 0.7144(6) 0.1063(3) 0.26739(14) 0.0691(10) Uani d . 1 . . C H15A 0.8075 0.0798 0.2943 0.104 Uiso calc R 1 . . H H15B 0.7899 0.147 0.241 0.104 Uiso calc R 1 . . H H15C 0.6466 0.0454 0.2506 0.104 Uiso calc R 1 . . H C16 0.4108(4) 0.2090(2) 0.20434(10) 0.0427(6) Uani d . 1 . . C H16 0.5084 0.1661 0.1869 0.051 Uiso calc R 1 . . H O1 0.1811(5) -0.15024(19) 0.07740(11) 0.0808(8) Uani d . 1 . . O O3 0.5046(5) -0.16511(18) 0.03935(9) 0.0726(7) Uani d . 1 . . O O5 0.8250(3) 0.22234(18) 0.04240(8) 0.0567(5) Uani d . 1 . . O O7 0.4771(5) 0.51390(17) 0.07818(10) 0.0722(7) Uani d . 1 . . O O8 0.1495(4) 0.50262(19) 0.10486(9) 0.0713(7) Uani d . 1 . . O O13 -0.0150(4) 0.39790(19) 0.28581(8) 0.0664(6) Uani d . 1 . . O O14 0.2866(4) 0.29970(18) 0.34039(7) 0.0615(6) Uani d . 1 . . O O15 0.5659(4) 0.1752(2) 0.29143(8) 0.0647(6) Uani d . 1 . . O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C2 0.105(3) 0.0383(18) 0.113(3) -0.008(2) -0.010(3) -0.015(2) C3A 0.076(2) 0.0333(15) 0.0491(15) 0.0050(17) -0.0024(15) -0.0062(12) C4 0.0602(19) 0.0469(17) 0.0446(14) 0.0085(16) 0.0030(14) -0.0045(13) C4A 0.0513(16) 0.0384(15) 0.0380(12) 0.0023(13) -0.0010(12) -0.0027(11) C5 0.0517(16) 0.0466(16) 0.0371(13) -0.0010(15) -0.0023(12) -0.0027(12) C5A 0.0575(17) 0.0391(15) 0.0408(13) -0.0051(14) 0.0006(12) -0.0034(12) C6 0.082(2) 0.0472(19) 0.071(2) -0.0079(19) 0.012(2) 0.0003(16) C8 0.079(2) 0.0388(17) 0.0477(16) 0.0044(19) -0.0054(16) -0.0037(13) C8A 0.0617(18) 0.0375(15) 0.0349(12) 0.0029(14) -0.0054(12) -0.0031(11) C9 0.0434(14) 0.0375(15) 0.0449(13) 0.0012(13) -0.0032(11) -0.0045(11) C9A 0.0495(16) 0.0370(15) 0.0400(13) 0.0015(14) -0.0056(12) -0.0023(11) C10 0.0555(17) 0.0432(17) 0.0568(16) -0.0026(15) 0.0023(14) -0.0047(13) C10A 0.070(2) 0.0367(16) 0.0575(17) -0.0091(16) -0.0045(16) -0.0023(13) C11 0.0431(13) 0.0322(14) 0.0441(13) -0.0034(12) 0.0022(11) -0.0010(11) C12 0.0450(14) 0.0373(15) 0.0481(14) 0.0017(13) -0.0007(12) -0.0005(12) C13 0.0521(16) 0.0363(16) 0.0526(15) -0.0006(14) 0.0082(13) -0.0076(12) C13A 0.060(2) 0.071(2) 0.083(2) 0.018(2) 0.0100(19) -0.0140(19) C14 0.0565(17) 0.0400(15) 0.0423(13) -0.0055(14) 0.0022(12) -0.0032(12) C14A 0.092(2) 0.081(3) 0.0531(17) 0.009(3) 0.0121(19) 0.0118(18) C15 0.0498(16) 0.0404(16) 0.0458(14) 0.0011(14) -0.0017(12) 0.0046(12) C15A 0.065(2) 0.072(2) 0.069(2) 0.023(2) -0.0089(18) 0.0082(18) C16 0.0449(14) 0.0386(15) 0.0447(13) 0.0065(13) 0.0039(11) 0.0000(12) O1 0.0935(18) 0.0400(13) 0.1090(19) -0.0135(14) 0.0064(16) -0.0126(13) O3 0.1007(19) 0.0381(12) 0.0792(15) 0.0078(14) 0.0064(15) -0.0140(11) O5 0.0533(11) 0.0637(14) 0.0532(10) -0.0043(12) 0.0059(10) -0.0082(10) O7 0.0936(18) 0.0359(12) 0.0870(16) -0.0020(13) 0.0085(16) -0.0005(11) O8 0.0914(18) 0.0474(14) 0.0753(15) 0.0230(15) -0.0043(14) -0.0062(11) O13 0.0717(15) 0.0680(15) 0.0596(12) 0.0249(14) 0.0089(12) -0.0127(11) O14 0.0795(15) 0.0624(14) 0.0427(10) -0.0008(13) -0.0014(10) -0.0089(10) O15 0.0703(14) 0.0737(16) 0.0501(11) 0.0218(13) -0.0076(10) 0.0026(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C2 O1 . 1.420(5) ? C2 O3 . 1.445(5) ? C2 H2A . 0.97 ? C2 H2B . 0.97 ? C3A C4 . 1.343(4) ? C3A O3 . 1.377(4) ? C3A C10A . 1.381(5) ? C4 C4A . 1.420(4) ? C4 H4 . 0.93 ? C4A C9A . 1.408(4) ? C4A C5 . 1.471(4) ? C5 O5 . 1.227(4) ? C5 C5A . 1.492(4) ? C5A C8A . 1.514(4) ? C5A C6 . 1.521(4) ? C5A H5A . 0.98 ? C6 O7 . 1.446(4) ? C6 H6A . 0.97 ? C6 H6B . 0.97 ? C8 O8 . 1.193(4) ? C8 O7 . 1.356(4) ? C8 C8A . 1.513(4) ? C8A C9 . 1.516(4) ? C8A H8A . 0.98 ? C9 C11 . 1.519(3) ? C9 C9A . 1.530(4) ? C9 H9 . 0.98 ? C9A C10 . 1.396(4) ? C10 C10A . 1.364(4) ? C10 H10 . 0.93 ? C10A O1 . 1.363(4) ? C11 C12 . 1.388(4) ? C11 C16 . 1.390(4) ? C12 C13 . 1.378(4) ? C12 H12 . 0.93 ? C13 O13 . 1.365(3) ? C13 C14 . 1.391(4) ? C13A O13 . 1.413(4) ? C13A H13A . 0.96 ? C13A H13B . 0.96 ? C13A H13C . 0.96 ? C14 O14 . 1.376(3) ? C14 C15 . 1.386(4) ? C14A O14 . 1.433(4) ? C14A H14A . 0.96 ? C14A H14B . 0.96 ? C14A H14C . 0.96 ? C15 O15 . 1.362(3) ? C15 C16 . 1.387(4) ? C15A O15 . 1.413(4) ? C15A H15A . 0.96 ? C15A H15B . 0.96 ? C15A H15C . 0.96 ? C16 H16 . 0.93 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 C2 O3 107.6(3) O1 C2 H2A 110.2 O3 C2 H2A 110.2 O1 C2 H2B 110.2 O3 C2 H2B 110.2 H2A C2 H2B 108.5 C4 C3A O3 128.6(3) C4 C3A C10A 121.7(3) O3 C3A C10A 109.6(3) C3A C4 C4A 117.9(3) C3A C4 H4 121 C4A C4 H4 121 C9A C4A C4 120.2(3) C9A C4A C5 121.9(2) C4 C4A C5 117.8(3) O5 C5 C4A 122.7(3) O5 C5 C5A 121.3(3) C4A C5 C5A 116.0(2) C5 C5A C8A 110.0(2) C5 C5A C6 119.6(2) C8A C5A C6 101.5(3) C5 C5A H5A 108.4 C8A C5A H5A 108.4 C6 C5A H5A 108.4 O7 C6 C5A 103.7(3) O7 C6 H6A 111 C5A C6 H6A 111 O7 C6 H6B 111 C5A C6 H6B 111 H6A C6 H6B 109 O8 C8 O7 122.3(3) O8 C8 C8A 129.7(3) O7 C8 C8A 107.9(3) C8 C8A C5A 102.3(3) C8 C8A C9 123.0(3) C5A C8A C9 112.5(2) C8 C8A H8A 106 C5A C8A H8A 106 C9 C8A H8A 106 C8A C9 C11 114.6(2) C8A C9 C9A 106.3(2) C11 C9 C9A 113.2(2) C8A C9 H9 107.5 C11 C9 H9 107.5 C9A C9 H9 107.5 C10 C9A C4A 119.8(3) C10 C9A C9 118.2(2) C4A C9A C9 122.0(2) C10A C10 C9A 117.9(3) C10A C10 H10 121 C9A C10 H10 121 O1 C10A C10 127.5(3) O1 C10A C3A 110.1(3) C10 C10A C3A 122.4(3) C12 C11 C16 119.4(2) C12 C11 C9 118.9(2) C16 C11 C9 121.8(2) C13 C12 C11 120.6(3) C13 C12 H12 119.7 C11 C12 H12 119.7 O13 C13 C12 124.5(3) O13 C13 C14 115.4(2) C12 C13 C14 120.1(3) O13 C13A H13A 109.5 O13 C13A H13B 109.5 H13A C13A H13B 109.5 O13 C13A H13C 109.5 H13A C13A H13C 109.5 H13B C13A H13C 109.5 O14 C14 C15 120.2(2) O14 C14 C13 120.3(3) C15 C14 C13 119.6(2) O14 C14A H14A 109.5 O14 C14A H14B 109.5 H14A C14A H14B 109.5 O14 C14A H14C 109.5 H14A C14A H14C 109.5 H14B C14A H14C 109.5 O15 C15 C14 115.4(2) O15 C15 C16 124.4(3) C14 C15 C16 120.3(3) O15 C15A H15A 109.5 O15 C15A H15B 109.5 H15A C15A H15B 109.5 O15 C15A H15C 109.5 H15A C15A H15C 109.5 H15B C15A H15C 109.5 C15 C16 C11 120.1(3) C15 C16 H16 119.9 C11 C16 H16 119.9 C10A O1 C2 105.5(3) C3A O3 C2 104.5(3) C8 O7 C6 111.3(2) C13 O13 C13A 118.4(2) C14 O14 C14A 111.6(2) C15 O15 C15A 118.3(2) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C6 H6A O8 1_655 0.97 2.57 3.531(5) 169 C9 H9 O5 1_455 0.98 2.37 3.254(3) 150 C8A H8A O5 3_455 0.98 2.26 3.220(3) 167 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag O3 C3A C4 C4A 177.6(3) ? C10A C3A C4 C4A 0.4(4) ? C3A C4 C4A C9A -0.6(4) ? C3A C4 C4A C5 -179.0(3) ? C9A C4A C5 O5 -176.5(2) ? C4 C4A C5 O5 1.8(4) ? C9A C4A C5 C5A 4.9(4) ? C4 C4A C5 C5A -176.8(2) ? O5 C5 C5A C8A 146.8(3) ? C4A C5 C5A C8A -34.5(3) ? O5 C5 C5A C6 30.1(4) ? C4A C5 C5A C6 -151.2(3) ? C5 C5A C6 O7 154.7(3) ? C8A C5A C6 O7 33.6(3) ? O8 C8 C8A C5A -158.8(3) ? O7 C8 C8A C5A 24.6(3) ? O8 C8 C8A C9 -31.3(5) ? O7 C8 C8A C9 152.0(3) ? C5 C5A C8A C8 -162.4(2) ? C6 C5A C8A C8 -34.8(3) yes C5 C5A C8A C9 63.8(3) yes C6 C5A C8A C9 -168.6(2) ? C8 C8A C9 C11 -54.3(4) ? C5A C8A C9 C11 68.6(3) ? C8 C8A C9 C9A 179.9(3) ? C5A C8A C9 C9A -57.2(3) ? C4 C4A C9A C10 0.6(4) ? C5 C4A C9A C10 178.8(2) ? C4 C4A C9A C9 -179.1(2) ? C5 C4A C9A C9 -0.8(4) ? C8A C9 C9A C10 -153.6(3) ? C11 C9 C9A C10 79.8(3) ? C8A C9 C9A C4A 26.1(3) ? C11 C9 C9A C4A -100.5(3) ? C4A C9A C10 C10A -0.3(4) ? C9 C9A C10 C10A 179.4(2) ? C9A C10 C10A O1 -176.9(3) ? C9A C10 C10A C3A 0.1(4) ? C4 C3A C10A O1 177.3(3) ? O3 C3A C10A O1 -0.4(4) ? C4 C3A C10A C10 -0.2(5) ? O3 C3A C10A C10 -177.8(3) ? C8A C9 C11 C12 87.0(3) ? C9A C9 C11 C12 -150.9(2) ? C8A C9 C11 C16 -92.8(3) ? C9A C9 C11 C16 29.3(3) ? C16 C11 C12 C13 0.3(4) ? C9 C11 C12 C13 -179.5(2) ? C11 C12 C13 O13 179.9(3) ? C11 C12 C13 C14 -0.5(4) ? O13 C13 C14 O14 -0.5(4) ? C12 C13 C14 O14 179.8(3) ? O13 C13 C14 C15 -179.9(3) ? C12 C13 C14 C15 0.4(4) ? O14 C14 C15 O15 1.1(4) ? C13 C14 C15 O15 -179.5(3) ? O14 C14 C15 C16 -179.7(3) ? C13 C14 C15 C16 -0.2(4) ? O15 C15 C16 C11 179.2(2) ? C14 C15 C16 C11 0.1(4) ? C12 C11 C16 C15 -0.1(4) ? C9 C11 C16 C15 179.7(3) ? C10 C10A O1 C2 -172.4(3) ? C3A C10A O1 C2 10.3(4) ? O3 C2 O1 C10A -16.1(4) ? C4 C3A O3 C2 173.0(3) ? C10A C3A O3 C2 -9.5(4) ? O1 C2 O3 C3A 15.7(4) ? O8 C8 O7 C6 180.0(3) ? C8A C8 O7 C6 -3.1(3) ? C5A C6 O7 C8 -19.7(3) ? C12 C13 O13 C13A 7.5(5) ? C14 C13 O13 C13A -172.1(3) ? C15 C14 O14 C14A -87.7(3) ? C13 C14 O14 C14A 92.9(3) ? C14 C15 O15 C15A 178.0(3) ? C16 C15 O15 C15A -1.2(4) ?